scholarly journals Evaluation of Pharmaceutical Quality of Mesalamine Delayed Release Tablets Using a New High Sensitivity Reversed-Phase UPLC Method for its Genotoxic/Aniline Impurity

2011 ◽  
Vol 8 (1) ◽  
pp. 167-179 ◽  
Author(s):  
Rakshit Kanubhai Trivedi ◽  
Mukesh C. Patel
Keyword(s):  
Detection Limit ◽  
Drug Product ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Limit Of Quantification ◽  
Release Formulation ◽  
Pharmaceutical Quality ◽  
Delayed Release ◽  
Run Time

A reversed phase ultra performance liquid chromatography (UPLC) method was developed and validated for the quantification of aniline in mesalamine delayed-release tablets. The optimization of the experimental condition was carried out considering some important requirements like, detection limit, short run time and reproducibility. In the present study, isocratic reversed-phase UPLC method was developed for determination and separation of aniline from the drug product. The drug and impurity are well separated by using a reversed phase (Reprosil Gold C18-XBD) column and mobile phase comprising of buffer pH 6.0 and acetonitrile in the ratio of 90:10 v/v. Other UPLC parameters which were optimised are flow rate, 0.5 mL/min; detection wavelength, 200 nm; column oven temperature, 50°C and injection volume 7 µL. Stability indicating capability was also established by forced degradation experiments. The method was validated as per ICH guideline. LOQ (limit of quantification) concentration (18 ng/mL) was found precise with RSD of less than 2%. In essence, the present study provides an improved low detection limit and lower run time for evaluation of pharmaceutical quality of mesalamine delayed-release formulation. Moreover, the developed method was also successfully applied for quantification of aniline in mesalamine delayed-release formulation. The same method can also be used for determination of aniline from drug substances.

scholarly journals Determination of Mesalamine Related Impurities from Drug Product by Reversed Phase Validated UPLC Method

2011 ◽  
Vol 8 (1) ◽  
pp. 131-148 ◽  
Author(s):  
Trivedi Rakshit Kanubhai ◽  
Patel Mukesh C ◽  
Kharkar Amit R
Keyword(s):  
Degradation Products ◽  
Drug Product ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Limit Of Quantification ◽  
Release Formulation ◽  
Delayed Release ◽  
Related Substances

In the present study gradient reversed-phase UPLC method was developed for simultaneous determination and separation of impurities and degradation products from drug product. The chromatographic separation was performed on acquity UPLC BEH C18 column (50 mm×2.1 mm, 1.7 µm) using gradient elution. Other UPLC parameters which were optimised are flow rate, 0.7 mL/min; detection wavelength, 220 nm; column oven temperature, 40°C and injection volume 7 µL. Stability indicating capability was established by forced degradation experiments and separation of known degradation products. The method was validated as per International Conference on Harmonization (ICH) guideline. For all impurities and mesalamine, LOQ (limit of quantification) value was found precise with RSD (related standard daviation) of less than 2.0%. In essence, the present study provides an improved low detection limit and lower run time for evaluation of pharmaceutical quality of mesalamine delayed-release formulation. Moreover, the developed method was successfully applied for quantification of impurities and degradation products in mesalamine delayed-release formulation. The same method can also be used for determination of related substances from mesalamine drug substance.

Quantification and In Silico Toxicity Assessment of Tazarotene and its Impurities for a Quality and Safe Drug Product Development

2019 ◽  
Vol 57 (7) ◽  
pp. 625-635 ◽  
Author(s):  
NVVSS Narayana Murty Nagulakonda ◽  
Ravi Shekar Ananthula ◽  
T Krishnamurthy ◽  
Muguda Ravi Prasada Rao ◽  
Gollapalli Nageswara Rao
Keyword(s):  
Product Development ◽  
In Silico ◽  
Limit Of Detection ◽  
Drug Product ◽  
Acne Vulgaris ◽  
Toxicity Assessment ◽  
Limit Of Quantification ◽  
Related Substances ◽  
In Silico Toxicity

Abstract Tazarotene is internationally accepted common name for ethyl 6-[(4,4-dimethylthiochroman-6-yl)ethynyl]nicotinate. It is a synthetic retinoid used for the topical treatment of mild to moderate plaque psoriasis, acne vulgaris and photo aging. To ensure the quality of drug product and drug substance, a LC–MS compatible UHPLC method was developed for quantification of drug and its related substances. Stationary phase with fused core particle technology is used for the separation of impurities. Limit of quantification and limit of detection of the method are 0.1 and 0.03%, respectively. Precision of the method for Tazarotene and all its related substances is less than 2.2% RSD. The correlation coefficient is >0.999. Accuracy of method is ranged from 95.3% to 107.0%. Application of this method in stability analysis has been demonstrated by analyzing stressed samples. Experimental design is used for the verification of robustness of the method. To ensure the safety, an in silico toxicity of the drug and its related substances were determined using TOPKAT and DEREK toxicity predictions Both UHPLC and in silico methods were validated as per the ICH Q2 and ICH M7 guidelines, which will enable a rapid product development of Tazarotene topical formulations while ensuring the safety and quality of product.

Pharmaceutical quality of docetaxel generics versus originator drug product: a comparative analysis

2008 ◽  
Vol 24 (7) ◽  
pp. 2019-2033 ◽  
Author(s):  
Jérôme Vial ◽  
Mélanie Cohen ◽  
Patrick Sassiat ◽  
Didier Thiébaut
Keyword(s):  
Comparative Analysis ◽  
Drug Product ◽  
Pharmaceutical Quality

scholarly journals A Stability Indicating UPLC Method for the Determination of Tramadol Hydrochloride: Application to Pharmaceutical Analysis

2012 ◽  
Vol 2012 ◽  
pp. 1-9 ◽  
Author(s):  
Kanakapura B. Vinay ◽  
Hosakere D. Revanasiddappa ◽  
Cijo M. Xavier ◽  
Pavagada J. Ramesh ◽  
Madihalli S. Raghu
Keyword(s):  
Limit Of Detection ◽  
Potassium Dihydrogen Phosphate ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Tramadol Hydrochloride ◽  
Stability Indicating

The use of Ultra Performance Liquid Chromatography (UPLC), with a rapid 5-minute reversed phase isocratic separation on a 1.7 μm reversed-phase packing material to provide rapid ‘‘high throughput’’ support for tramadol hydrochloride (TMH) is demonstrated. A simple, precise and accurate stability-indicating isocratic UPLC method was developed for the determination of TMH in bulk drug and in its tablets. The method was developed using Waters Aquity BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with mobile phase consisting of a mixture of potassium dihydrogen phosphate buffer of pH 2.8 and an equal volume of acetonitrile (60 : 40 v/v). The eluted compound was detected at 226 nm with a UV detector. The standard curve of mean peak area versus concentration showed an excellent linearity over a concentration range 0.5–300 μg mL−1 TMH with regression coefficient (r) value of 0.9999. The limit of detection (S/N =3) was 0.08 μg mL−1 and the limit of quantification (S/N =10) was 0.2 μg mL−1. Forced degradation of the bulk sample was conducted an accordance with the ICH guidelines. Acidic, basic, hydrolytic, oxidative, thermal and photolytic degradation were used to assess the stability indicating power of the method. TMH was found to degrade significantly in acidic, basic and oxidative stress conditions and stable in thermal, hydrolytic and photolytic conditions.

scholarly journals A New Validated Stability indicating RP-HPLC Method for Simultaneous Quantification of Impurities of Fluticasone Propionate and Salmeterol Xenafoate in Metered Dose Inhalation Aerosol

2021 ◽  
Vol 33 (4) ◽  
pp. 867-872
Author(s):  
Surya Prakash Mamillapalli ◽  
Shirisha Koyya ◽  
B. Venkata Subbaiah ◽  
N. Annapurna
Keyword(s):  
Fluticasone Propionate ◽  
Drug Product ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Simultaneous Quantification ◽  
Metered Dose ◽  
Dose Inhalation

A simple, specific, precise, accurate and stability indicating reversed phase HPLC method for simultaneous quantification of total 12 impurities of fluticasone propionate and salmeterol xenafoate in metered dose inhalation aerosol has been developed in the present work. Chromatographic separation between impurities of both compounds were achieved on Altima C18 250 × 4.6 mm, 5 μ column using a step-gradient elution at a flow rate of 1.4 mL/min, 0.1% v/v orthophosphoric acid as buffer and acetonitrile as mobile phase constituents. Forced degradation studies for drug product were performed and revealed that Salmeterol is acid sensitive (about 21.3%), degrades to IMP-D and fluticasone is alkali sensitive (about 7.6%) and degrades to IMP-A. All degradant and process related impurities of both compounds were monitored at 214 nm and spectral purity along with % mass balance is assessed using PDA detector, which proved stability indicating capability of the method. The developed method is fully validated as per current ICH guidelines, where precision is achieved at % RSD of < 5, Correlation of < 0.999 for linearity, LOD-LOQ at < 0.02% and < 0.05%, along with satisfactory system suitability results under robustness conditions.

Development and Validation of a Reversed-Phase Ultra-Performance Liquid Chromatographic Method for Assay of Lacidipine and Related Substances

2011 ◽  
Vol 94 (6) ◽  
pp. 1800-1806 ◽  
Author(s):  
Arivozhi Mohan ◽  
Hitesh B Patel ◽  
Dhandayutham Saravanan
Keyword(s):  
Degradation Products ◽  
Drug Product ◽  
Reversed Phase ◽  
Drug Substance ◽  
Forced Degradation ◽  
Related Substances ◽  
Forced Degradation Studies ◽  
Acetic Acid Buffer ◽  
Development And Validation ◽  
Liquid Chromatographic

Abstract A simple isocratic, RP-ultra-performance LC method was developed and validated for the determination of lacidipine, three process impurities formed during synthesis, and three degradation products present in drug substance and the drug product. An efficient chromatographic separation was achieved on an Acquity BEH C18 column using pH 4.5 ammonium acetate–acetic acid buffer–methanol (70 + 30, v/v) mobile phase. The monitoring wavelength was 240 nm, and the flow rate 0.25 mL/min. Forced degradation studies using acid, alkali, peroxide, water, heat, and light were conducted, and all impurities were separated. The method was validated successfully for specificity, precision, linearity, accuracy, LOD, LOQ, and robustness, according to International Conference on Harmonization guidelines. The linearity of the calibration curve for lacidipine and each impurity was found to be very good (r2 &gt; 0.999). This method is shown to be suitable for analysis of lacidipine to evaluate the quality of drug substance and a drug product.

scholarly journals DEVELOPMENT OF A NEW STABILITY INDICATING RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF EPALRESTAT AND PREGABALIN AND ITS VALIDATION AS PER INTERNATIONAL CONFERENCE ON HARMONIZATION GUIDELINES

2018 ◽  
Vol 11 (5) ◽  
pp. 319
Author(s):  
Swapna Goday ◽  
Abdul Rahaman Sk ◽  
Prameelarani A
Keyword(s):  
Retention Time ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
International Conference ◽  
Stability Indicating

Objective: The present study was aimed to develop a novel, simple, rapid, accurate, stability-indicating reversed-phase high-performance liquid chromatography method, and validate for the simultaneous estimation of epalrestat and pregabalin in bulk and dosage form. Methods: The chromatographic separation was performed on c18 column discovery (250 mm × 4.6 mm, 5 μ particle size) the optimized mobile phase consists of 0.01 m potassium dihydrogen phosphate buffer: Methanol (25:75% v/v) with a flow rate of 1.0 ml/min and ultraviolet (UV) detection at 226 nm. Results: The chromatographic condition, retention time was 2.2 min (pregabalin), 2.8 min (epalrestat). Stress testing was performed in accordance with an International Conference on Harmonization (ICH) Q1A R2 guidelines. The method was validated as per ICH Q2 R1 guidelines. Linearity range was 30–180 ppm (epalrestat), 15–90 ppm (pregabalin), accuracy was in the range of 98.14–100.43% for both the drugs. Precision was 0.2% and 0.3% for epalrestat and pregabalin. Limit of detection and limit of quantification are 0.21 μg/ml and 0.65 μg/ml for epalrestat and 0.08 μg/ml and 0.25 μg/ml for pregabalin. Conclusion: The method developed is more sensitive, accurate, and precise than the methods reported earlier. Retention time and runtime were also less, and hence, the method is economical. When applied for tablet assay, drug content was within 100.06–100.22% of the labeled content. Forced degradation studies indicated the suitability of the method for stability studies. The proposed method can be used for routine determination of epalrestat and pregabalin.

scholarly journals Development and Validation of Stability-Indicating RP-UPLC Method for the Determination of Methdilazine in Bulk Drug and in Pharmaceutical Dosage Form

2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Madihalli S. Raghu ◽  
Kanakapura Basavaiah ◽  
Cijo M. Xavier ◽  
Kudige N. Prashanth
Keyword(s):  
Limit Of Detection ◽  
Bulk Sample ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Bulk Drug

A simple, precise, and accurate, and stability-indicating isocratic Ultraperformance Liquid Chromatography (UPLC) method was developed for the determination of methdilazine hydrochloride (MDH) in bulk drug and in its tablets. The use of UPLC, with a rapid 5-minute-reversed-phase isocratic separation on a 1.7 μm reversed-phase packing material to provide rapid ‘‘high throughput’’ support for MDH, is demonstrated. The method was developed using Waters Acquity BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with mobile phase consisting of a mixture of potassium dihydrogenorthophosphate and 1-pentane sulphonic acid buffer of pH 4.0 and acetonitrile (60 : 40 v/v). The eluted compound was detected at 254 nm with a UV detector. The standard curve of mean peak area versus concentration showed an excellent linearity over a concentration range 0.5–80 μg mL−1 MDH with regression coefficient () value of 0.9999. The limit of detection () was 0.2 μg mL−1 and the limit of quantification () was 0.5 μg mL−1. Forced degradation of the bulk sample was conducted in accordance with the ICH guidelines. Acidic, basic, hydrolytic, oxidative, thermal, and photolytic degradations were used to assess the stability indicating power of the method. The drug was found to be stable in acidic, basic, thermal, hydrolytic, and photolytic stress conditions and showed slight degradation in oxidative stress condition.

Pharmaceutical quality of yarrow (Achillea millefolium L. s.l.) – Investigation of 40 commercial drug samples by means of the bioactive compounds

Planta Medica ◽  
2007 ◽  
Vol 73 (09) ◽  
Author(s):  
B Benedek ◽  
K Rothwangl-Wiltschnigg ◽  
E Rozema ◽  
N Gjoncaj ◽  
G Reznicek ◽  
...  
Keyword(s):  
Bioactive Compounds ◽  
Achillea Millefolium ◽  
Pharmaceutical Quality

System errors of manufacturers of medicines detected by conducting of state control in the area of circulation of medicines

2019 ◽  
Vol 2019 (5) ◽  
pp. 32-38
Author(s):  
Валентина Косенко ◽  
Valentina Kosenko ◽  
Алла Трапкова ◽  
Alla Trapkova ◽  
Светлана Тарасова ◽  
...  
Keyword(s):  
Quality Control ◽  
Quality Management ◽  
Management Systems ◽  
State Control ◽  
Quality Management Systems ◽  
Conducting State ◽  
Pharmaceutical Quality ◽  
State Quality ◽  
System Errors

The article conducts the analysis of system errors detected by Roszdravnadzor by conducting state quality control of circulating medicines, as well as weaknesses in pharmaceutical quality management systems of the manufacturers, that can influence the quality of manufactured drugs.

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